Surfactant removal from the surface of platinum-based nanoparticles prepared using solution-based methods is a prerequisite to realize their high catalytic performance for electrochemical reactions. Herein, we report an effective approach combining acetic acid refluxing with an electrochemical process for the removal of amine-or thiol-based capping agents from the surface of supported-platinum nanoparticles. This strategy involves surfactant protonation by refluxing the supported-platinum particles in acetic acid followed by surfactant removal by subsequent electrochemical treatment at high potential. We demonstrate that this combined activation process is essential to enhance platinum particle performance in catalyzing direct methanol fuel cell reactions, including methanol oxidation and oxygen reduction reactions. The studies in this work show promise in electrocatalysis applications of solution-based materials synthesis. (C) 2016 Chinese Society of Particuology and Institute of Process Engineering, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.